#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/80/7008059.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7008059
loop_
_publ_author_name
'Lazarides, Theodore'
'Miller, Thomas A.'
'Jeffery, John C.'
'Ronson, Tanya K.'
'Adams, Harry'
'Ward, Michael D.'
_publ_section_title
;
 Luminescent complexes of Re(I) and Ru(II) with appended macrocycle
 groups derived from 5,6-dihydroxyphenanthroline: cation and anion
 binding.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              528
_journal_page_last               536
_journal_paper_doi               10.1039/b416293e
_journal_year                    2005
_chemical_formula_sum            'C25 H27 Cl N2 O9.5 Re'
_chemical_formula_weight         729.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.9390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.0812(17)
_cell_length_b                   16.5695(11)
_cell_length_c                   12.9281(9)
_cell_measurement_temperature    173(2)
_cell_volume                     5360.0(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27774
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    4.691
_exptl_absorpt_correction_T_max  0.61
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.071
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6176
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0333P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                4380
_reflns_number_total             6176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b416293e.txt
_cod_data_source_block           gingerm
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C25 H27 Cl N2 O9.50 Re'
_cod_database_code               7008059
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re Re 1.138449(7) 0.132432(10) -0.002595(13) 0.03139(6) Uani 1 1 d D . .
Cl Cl 1.12103(9) 0.09147(12) 0.17488(15) 0.0341(4) Uani 0.82 1 d PDU A 1
C31 C 1.1478(7) 0.1655(9) -0.1413(10) 0.041(3) Uani 0.82 1 d PDU A 1
O31 O 1.1522(2) 0.1858(4) -0.2266(4) 0.0575(17) Uani 0.82 1 d PDU A 1
ClA Cl 1.1420(8) 0.1825(10) -0.1745(10) 0.042(3) Uani 0.18 1 d PDU A 2
C31A C 1.127(2) 0.089(2) 0.1317(17) 0.056(11) Uani 0.18 1 d PDU A 2
O31A O 1.1268(9) 0.0645(14) 0.2155(11) 0.040(6) Uani 0.18 1 d PDU A 2
C30 C 1.15420(19) 0.0238(3) -0.0412(4) 0.0383(11) Uani 1 1 d . A .
O30 O 1.16300(14) -0.0428(2) -0.0595(3) 0.0511(9) Uani 1 1 d . . .
C32 C 1.2132(2) 0.1490(3) 0.0316(4) 0.0399(11) Uani 1 1 d . A .
O32 O 1.25808(15) 0.1598(2) 0.0495(3) 0.0542(10) Uani 1 1 d . . .
N1 N 1.05244(14) 0.1280(2) -0.0360(2) 0.0297(8) Uani 1 1 d . A .
N2 N 1.11059(14) 0.2480(2) 0.0526(2) 0.0298(8) Uani 1 1 d . A .
C1 C 1.14018(18) 0.3079(2) 0.0959(3) 0.0310(10) Uani 1 1 d . . .
H1 H 1.1772 0.3034 0.0988 0.037 Uiso 1 1 calc R A .
C2 C 1.11751(19) 0.3773(3) 0.1370(3) 0.0354(10) Uani 1 1 d . A .
H2 H 1.1394 0.4178 0.1661 0.042 Uiso 1 1 calc R . .
C3 C 1.06326(19) 0.3853(2) 0.1341(3) 0.0333(10) Uani 1 1 d . . .
H3 H 1.0479 0.4310 0.1611 0.040 Uiso 1 1 calc R A .
C4 C 1.03088(18) 0.3231(2) 0.0896(3) 0.0297(10) Uani 1 1 d . A .
C5 C 1.05646(16) 0.2557(2) 0.0499(3) 0.0273(9) Uani 1 1 d . . .
C6 C 1.02538(17) 0.1927(2) 0.0009(3) 0.0273(9) Uani 1 1 d . A .
C7 C 0.96915(17) 0.1978(2) -0.0080(3) 0.0303(10) Uani 1 1 d . . .
C8 C 0.94084(18) 0.1364(3) -0.0632(3) 0.0340(9) Uani 1 1 d . A .
H8 H 0.9037 0.1383 -0.0718 0.041 Uiso 1 1 calc R . .
C9 C 0.96813(19) 0.0741(3) -0.1043(4) 0.0376(11) Uani 1 1 d . . .
H9 H 0.9500 0.0340 -0.1428 0.045 Uiso 1 1 calc R A .
C10 C 1.02353(19) 0.0716(3) -0.0874(3) 0.0350(10) Uani 1 1 d . A .
H10 H 1.0415 0.0279 -0.1138 0.042 Uiso 1 1 calc R . .
C11 C 0.97371(18) 0.3267(3) 0.0824(3) 0.0305(10) Uani 1 1 d . . .
C12 C 0.94389(18) 0.2663(3) 0.0373(3) 0.0324(10) Uani 1 1 d . A .
O13 O 0.88936(12) 0.26869(19) 0.0301(2) 0.0368(7) Uani 1 1 d . . .
C14 C 0.86738(18) 0.2446(3) 0.1265(3) 0.0378(11) Uani 1 1 d . A .
H14B H 0.8876 0.2696 0.1846 0.045 Uiso 1 1 calc R . .
H14A H 0.8700 0.1865 0.1346 0.045 Uiso 1 1 calc R . .
C15 C 0.81018(18) 0.2701(3) 0.1254(4) 0.0434(12) Uani 1 1 d . . .
H15B H 0.7919 0.2564 0.0592 0.052 Uiso 1 1 calc R A .
H15A H 0.7927 0.2419 0.1794 0.052 Uiso 1 1 calc R . .
O16 O 0.80752(13) 0.35390(19) 0.1418(3) 0.0499(9) Uani 1 1 d . A .
C17 C 0.7544(2) 0.3827(3) 0.1495(5) 0.0590(15) Uani 1 1 d . . .
H17B H 0.7357 0.3472 0.1943 0.071 Uiso 1 1 calc R A .
H17A H 0.7356 0.3820 0.0814 0.071 Uiso 1 1 calc R . .
C18 C 0.7544(3) 0.4651(5) 0.1914(6) 0.103(3) Uani 1 1 d . A .
H18B H 0.7687 0.5007 0.1404 0.123 Uiso 1 1 calc R . .
H18A H 0.7176 0.4808 0.1979 0.123 Uiso 1 1 calc R . .
O19 O 0.78024(17) 0.4784(3) 0.2784(4) 0.0891(15) Uani 1 1 d . . .
C20 C 0.7794(2) 0.5548(3) 0.3259(5) 0.0566(14) Uani 1 1 d . A .
H20B H 0.7839 0.5472 0.4004 0.068 Uiso 1 1 calc R . .
H20A H 0.7445 0.5785 0.3103 0.068 Uiso 1 1 calc R . .
C21 C 0.8203(2) 0.6131(3) 0.2956(4) 0.0525(14) Uani 1 1 d . . .
H21B H 0.8152 0.6245 0.2220 0.063 Uiso 1 1 calc R A .
H21A H 0.8167 0.6633 0.3332 0.063 Uiso 1 1 calc R . .
O22 O 0.87213(13) 0.57965(18) 0.3191(2) 0.0389(8) Uani 1 1 d . A .
C23 C 0.9151(2) 0.6319(3) 0.2968(3) 0.0418(11) Uani 1 1 d . . .
H23B H 0.9476 0.6119 0.3328 0.050 Uiso 1 1 calc R A .
H23A H 0.9081 0.6850 0.3243 0.050 Uiso 1 1 calc R . .
C24 C 0.9243(2) 0.6401(3) 0.1830(3) 0.0423(11) Uani 1 1 d . A .
H24B H 0.8912 0.6565 0.1458 0.051 Uiso 1 1 calc R . .
H24A H 0.9504 0.6823 0.1745 0.051 Uiso 1 1 calc R . .
O25 O 0.94259(13) 0.56715(18) 0.1385(2) 0.0410(8) Uani 1 1 d . . .
C26 C 0.89991(18) 0.5141(3) 0.1071(3) 0.0362(10) Uani 1 1 d . A .
H26B H 0.8736 0.5425 0.0622 0.043 Uiso 1 1 calc R . .
H26A H 0.8826 0.4953 0.1674 0.043 Uiso 1 1 calc R . .
C27 C 0.92137(19) 0.4441(3) 0.0508(3) 0.0359(11) Uani 1 1 d . . .
H27B H 0.8923 0.4139 0.0161 0.043 Uiso 1 1 calc R A .
H27A H 0.9446 0.4629 -0.0011 0.043 Uiso 1 1 calc R . .
O28 O 0.95111(13) 0.39295(18) 0.1256(2) 0.0357(7) Uani 1 1 d . A .
O40 O 0.0000 0.0879(6) 0.2500 0.164(4) Uani 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C31 Re C30 89.1(5) . . ?
C31 Re C32 89.7(5) . . ?
C30 Re C32 88.78(19) . . ?
C31 Re C31A 174.4(14) . . ?
C30 Re C31A 85.9(13) . . ?
C32 Re C31A 92.7(15) . . ?
C31 Re N1 90.4(5) . . ?
C30 Re N1 97.83(17) . . ?
C32 Re N1 173.39(16) . . ?
C31A Re N1 87.8(15) . . ?
C31 Re N2 96.8(4) . . ?
C30 Re N2 171.43(16) . . ?
C32 Re N2 97.43(16) . . ?
C31A Re N2 87.9(13) . . ?
N1 Re N2 75.99(13) . . ?
C31 Re ClA 6.0(8) . . ?
C30 Re ClA 93.6(4) . . ?
C32 Re ClA 93.8(5) . . ?
C31A Re ClA 173.5(16) . . ?
N1 Re ClA 85.8(5) . . ?
N2 Re ClA 91.9(4) . . ?
C31 Re Cl 176.8(5) . . ?
C30 Re Cl 92.10(14) . . ?
C32 Re Cl 93.33(14) . . ?
C31A Re Cl 6.2(13) . . ?
N1 Re Cl 86.47(10) . . ?
N2 Re Cl 81.69(10) . . ?
ClA Re Cl 171.0(4) . . ?
O31 C31 Re 178.3(15) . . ?
O31A C31A Re 172(4) . . ?
O30 C30 Re 176.5(4) . . ?
O32 C32 Re 178.2(4) . . ?
C10 N1 C6 117.1(4) . . ?
C10 N1 Re 128.5(3) . . ?
C6 N1 Re 114.4(3) . . ?
C1 N2 C5 117.7(4) . . ?
C1 N2 Re 127.5(3) . . ?
C5 N2 Re 114.6(3) . . ?
N2 C1 C2 122.6(4) . . ?
C3 C2 C1 119.9(4) . . ?
C2 C3 C4 119.1(4) . . ?
C5 C4 C3 117.8(4) . . ?
C5 C4 C11 119.4(4) . . ?
C3 C4 C11 122.9(4) . . ?
N2 C5 C4 123.0(4) . . ?
N2 C5 C6 117.2(4) . . ?
C4 C5 C6 119.7(4) . . ?
N1 C6 C7 122.3(4) . . ?
N1 C6 C5 117.3(4) . . ?
C7 C6 C5 120.4(4) . . ?
C8 C7 C6 117.8(4) . . ?
C8 C7 C12 123.6(4) . . ?
C6 C7 C12 118.6(4) . . ?
C9 C8 C7 119.6(4) . . ?
C8 C9 C10 118.9(4) . . ?
N1 C10 C9 124.1(4) . . ?
C12 C11 O28 122.3(4) . . ?
C12 C11 C4 121.2(4) . . ?
O28 C11 C4 116.5(4) . . ?
C11 C12 O13 121.9(4) . . ?
C11 C12 C7 120.7(4) . . ?
O13 C12 C7 117.4(4) . . ?
C12 O13 C14 111.8(3) . . ?
O13 C14 C15 109.6(4) . . ?
O16 C15 C14 109.4(4) . . ?
C15 O16 C17 113.3(4) . . ?
O16 C17 C18 111.1(5) . . ?
O19 C18 C17 118.2(6) . . ?
C18 O19 C20 121.2(6) . . ?
O19 C20 C21 116.2(5) . . ?
O22 C21 C20 109.1(4) . . ?
C23 O22 C21 114.3(4) . . ?
O22 C23 C24 114.8(4) . . ?
O25 C24 C23 113.0(4) . . ?
C26 O25 C24 112.4(4) . . ?
O25 C26 C27 109.3(4) . . ?
O28 C27 C26 108.4(3) . . ?
C11 O28 C27 113.8(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re C31 1.905(12) . ?
Re C30 1.916(5) . ?
Re C32 1.916(5) . ?
Re C31A 1.918(19) . ?
Re N1 2.172(3) . ?
Re N2 2.176(3) . ?
Re ClA 2.379(11) . ?
Re Cl 2.4604(19) . ?
C31 O31 1.165(12) . ?
C31A O31A 1.158(18) . ?
C30 O30 1.154(5) . ?
C32 O32 1.147(6) . ?
N1 C10 1.332(5) . ?
N1 C6 1.372(5) . ?
N2 C1 1.339(5) . ?
N2 C5 1.362(5) . ?
C1 C2 1.403(6) . ?
C2 C3 1.365(6) . ?
C3 C4 1.410(6) . ?
C4 C5 1.403(6) . ?
C4 C11 1.432(6) . ?
C5 C6 1.425(5) . ?
C6 C7 1.409(6) . ?
C7 C8 1.406(6) . ?
C7 C12 1.444(6) . ?
C8 C9 1.366(6) . ?
C9 C10 1.392(6) . ?
C11 C12 1.356(6) . ?
C11 O28 1.372(5) . ?
C12 O13 1.365(5) . ?
O13 C14 1.453(5) . ?
C14 C15 1.495(6) . ?
C15 O16 1.407(5) . ?
O16 C17 1.424(6) . ?
C17 C18 1.469(8) . ?
C18 O19 1.278(7) . ?
O19 C20 1.407(6) . ?
C20 C21 1.480(7) . ?
C21 O22 1.427(6) . ?
O22 C23 1.427(5) . ?
C23 C24 1.510(6) . ?
C24 O25 1.428(5) . ?
O25 C26 1.422(5) . ?
C26 C27 1.489(6) . ?
C27 O28 1.453(5) . ?
